EP0937784B1 - Verfahren zur Wiederherstellung von Eigenschaften einer hitzebeständigen Legierung auf Nickelbasis - Google Patents

Verfahren zur Wiederherstellung von Eigenschaften einer hitzebeständigen Legierung auf Nickelbasis Download PDF

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Publication number
EP0937784B1
EP0937784B1 EP99301222A EP99301222A EP0937784B1 EP 0937784 B1 EP0937784 B1 EP 0937784B1 EP 99301222 A EP99301222 A EP 99301222A EP 99301222 A EP99301222 A EP 99301222A EP 0937784 B1 EP0937784 B1 EP 0937784B1
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alloy
subjected
hours
test
temperature
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French (fr)
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EP0937784A1 (de
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Hisataka c/o Takasago Machinery Works Kawai
Yoshinao c/o Takasago Res. & Dev. Center Hibaru
Ikuo c/o Takasago Res. & Dev. Center Okada
Takayuki c/o Takasago Res. & Dev. Center Imazu
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Mitsubishi Heavy Industries Ltd
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Mitsubishi Heavy Industries Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P6/00—Restoring or reconditioning objects
    • B23P6/002—Repairing turbine components, e.g. moving or stationary blades, rotors
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

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  • the present invention relates to a property recovering method for a Ni-base heat resistant alloy whose properties such as strength and ductility have been deteriorated by the use at a high temperature.
  • a Ni-base heat resistant alloy which has a ⁇ ' intermetallic compound of Ni 3 (Al, Ta, Ti) as a main ingredient and also has a solid solution strengthening function given by precipitation hardening of the second phase and Mo, W, or the like has been used for a high-temperature member such as a moving blade of gas turbine and jet engine.
  • the second phase is a phase containing an intermetallic compound, carbide, and the like.
  • the aforesaid Ni-base heat resistant alloys include a Ni-base heat resistant alloy disclosed in Japanese Patent Provisional Publication No. 6-57359 (No.
  • alloy A a Ni-base heat resistant alloy commercially available under the tradename Inconel 738 (hereinafter referred to as alloy B).
  • alloy B a Ni-base heat resistant alloy commercially available under the tradename Inconel 738
  • the second phase (intermetallic compound, carbide, etc.) is coarsened or the diffusion and condensation of impurity elements take place because of heat history due to the long-term use at a high temperature, by which the strength and ductility are decreased. Therefore, the member using such an alloy becomes incapable of being used, and finally must be scrapped because of the formation of cracks. Also, these Ni-base heat resistant alloys are generally very expensive.
  • the present invention has been made in view of the aforementioned situation of the prior art, and accordingly an object of the present invention is to provide a property recovering method which can be applied to a high-temperature member such as a blade member that must be scrapped due to the deterioration of properties such as strength and ductility caused by the long-term use at a high temperature to recover its properties to those before the use, enable its reuse, and contribute to the effective use of resources and the conservation of environment.
  • the inventors have earnestly studied a property recovering method for a Ni-base heat resistant alloy whose properties have been deteriorated by the long-term use at a high temperature. As a result, we found that the properties can be recovered by performing two-stage solution treatment at a predetermined temperature on the alloy having deteriorated properties and then by performing aging treatment thereon, and completed the present invention.
  • a first mode of the present invention is a property recovering method for a Ni-base heat resistant alloy, in which a Ni-base heat resistant alloy containing, in percent by weight, 13.1-15% Cr, 8.5-10.5% Co, 1-3.5% Mo, 3.5-4.5% W, 3-5.5% Ta, 3.5-4.5% Al, 2.2-3.2% Ti, 0.06-0.12% C, 0.025% or less B, 0.01-0.05% Zr, 1-100 ppm Mg and/or Ca, and 0-1.5% Hf, the balance being Ni and unavoidable impurities, whose properties have been deteriorated by heat history, is subjected to first-stage solution treatment, in which the alloy is held at a temperature of 1175 to 1225°C for 1 to 5 hours and then furnace-cooled, then subjected to second-stage solution treatment, in which the alloy is held at a temperature of 1115 to 1165°C for 1 to 5 hours and then air-cooled, and further subjected to aging treatment, in which the alloy is held at a
  • a second mode of the present invention is a property recovering method for a Ni-base heat resistant alloy, in which a Ni-base heat resistant alloy containing, in percent by weight, 15.7-16.3% Cr, 8-9% Co, 1.5-2% Mo, 2.4-2.8% W, 1.5-2% Ta, 3.2-3.7% Al, 3.2-3.7% Ti, 0.09-0.13% C, 0.007-0.012% B, 0.03-0.08% Zr, 0.6-1.1% Nb, 0.05% or less Fe, 0.02% or less Mn, 0.3% or less Si, and 0.015% or less S (where Al + Ti: 6.5-7.2%), the balance being Ni and unavoidable impurities, whose properties have been deteriorated by heat history, is subjected to first-stage solution treatment, in which the alloy is held at a temperature of 1175 to 1225°C for 1 to 5 hours and then furnace-cooled, then subjected to second-stage solution treatment, in which the alloy is held at a temperature of 1115 to 1165°C for 1 to 5 hours
  • the properties of a Ni-base heat resistant alloy whose properties such as strength and ductility have been deteriorated by the second phase coarsened by heat history can be recovered to the state before being subjected to heat history.
  • the present invention enables the reuse of a member that had to be scrapped conventionally, and can contribute to the saving and effective use of expensive metallic elements and further to the conservation of environment.
  • Ni-base heat resistant alloys whose properties have been deteriorated by receiving heat history, subjected to property recovering treatment in accordance with the present invention are the Ni-base heat resistant alloy described in Japanese Patent Provisional Publication No. 6-57359 (No. 57359/1994) (alloy A) and the Ni-base heat resistant alloy commercially available under the tradename Inconel 738 (alloy B). Their compositions are in the range of chemical component shown in the aforementioned Table 1.
  • General heat treatment conditions in manufacturing are as follows: After being held at 1120°C for two hours, the alloy is air-cooled to room temperature. Thereafter, it is held at 850°C for 24 hours, and then air-cooled to room temperature (hereinafter indicated by 1120°C x 2h/air cooling + 850°C x 24h/air cooling).
  • Ni-base heat resistant alloys are heated for a long period of time in a temperature range of 700 to 1000°C, which is a normal service temperature of high-temperature members for which these alloys are used, the second phase (including intermetallic compound and carbide) deposited at grain boundaries and in the grains grows and coarsens, so that the strength and ductility are decreased which results in the member having to be scrapped also because of crack formation. Therefore, in accordance with the method of the present invention, a first-stage solution treatment is applied, in which the alloy is held at a temperature of 1175 to 1225°C for 1 to 5 hours and is then furnace cooled.
  • the alloy is then subjected to a second-stage solution treatment, in which the alloy is held at a temperature of 1115 to 1165°C for 1 to 5 hours and is then air-cooled.
  • the alloy is finally subjected to an ageing treatment in which the alloy is held at a temperature of 810 to 860°C for 22 to 26 hours.
  • the holding time of heating temperature depends on the size of member and the situation of furnace. However, if the holding time is 1 hour or shorter, the elements are not diffused sufficiently, so that the recovery of properties is insufficient. If the holding time is increased to 5 hours or longer, the recovery shows a saturating state. Therefore, the proper holding time is 1 to 5 hours considering the cost.
  • the second-stage solution treatment and aging treatment are processes for re-depositing the second phase.
  • the second phase becomes coarse or fine, so that the strength and ductility equal to those of unused (unheated) material cannot be obtained.
  • the second-stage solution treatment and aging treatment must be performed under proper conditions.
  • a proper temperature for the second-stage solution treatment is 1140 ⁇ 25°C (1115 to 1165°C), and a proper temperature for the aging treatment is 835 ⁇ 25°C (810 to 860°C), which is generally used from the previous experience.
  • a proper holding time is 1 to 5 hours for the second-stage solution treatment and 24 ⁇ 2 hours (22 to 26 hours) for the aging treatment.
  • Round bars (diameter: 15 mm, length: 90 mm) of alloy A and alloy B having chemical compositions shown in Table 2 were used as experimental materials.
  • the materials (test materials of Nos. 2 and 9) whose properties have been deteriorated by heating at 900°C for 10,000 hours were subjected to the first-stage solution treatment or the second-stage solution treatment and then the aging treatment.
  • Five types of reheated materials (test materials Nos. 3 to 7) for alloy A and two types of re-heat treated materials (test materials Nos. 10 and 11) for alloy B were prepared.
  • the holding time for solution treatment was constant, being 2 hours, and only the heating temperature for the first-stage solution treatment was made an experimental parameter.
  • the aging treatment was performed under the same conditions of 850°C and 24 hours.
  • test materials Nos. 3 to 7, and 10 and 11 On the re-heat treated materials (test materials Nos. 3 to 7, and 10 and 11), unheated materials (test materials Nos. 1 and 8), and long-term heated materials (test materials Nos. 2 and 9) heated at 900°C for 10,000 hours, microstructure, hardness, tensile, and creep rupture tests were conducted.
  • Table 3 collectively shows the classification of the used test materials, re-heat treatment conditions, and the like. Also, the test results are shown in FIGS. 1 to 6 and Tables 4 to 7.
  • Test material No. 2 is treated under condition of 1150°C ⁇ 2h/furnace cooling + 1120°C ⁇ 2h/air cooling + 850°C ⁇ 24h/air cooling.
  • Material of the present invention Test material No. 2 is treated under condition of 1200°C ⁇ 2h/furnace cooling + 1120°C ⁇ 2h/air cooling + 850°C ⁇ 24h/air cooling.
  • Alloy B 8 Unheated material Heat treatment (1120°C ⁇ 2h/air cooling + 850°C ⁇ 24h/air cooling) in manufacturing
  • Long-term heated material Unheated material (test material No. 8) is treated under condition 900°C x 10000h. 10 Re-heat treted material Comparative material Test material No.
  • Test material No. 9 is treated under condition of 1200°C x 2h/furnace cooling + 1120°C X 2h/air cooling + 850°C ⁇ 24h/air cooling.
  • the hardness was HV420, and the tensile strength and elongation at room temperature were 114.3 kg/mm 2 and 7.1%, respectively.
  • the hardness decreased to HV362, and the tensile strength and elongation at room temperature decreased to 83.5 kg/mm 2 and 2.2%, respectively.
  • the 0.2% proof stress and the reduction of area at room temperature and the 0.2% proof stress, tensile strength, elongation, and reduction of area at 650°C also decreased as compared with those of the unheated material.
  • FIGS 2 and 3 are microphotographs of X5000 magnification showing microstructures of test materials.
  • FIG. 2 shows the microstructure of unheated material (test material No. 1) and
  • FIG. 3 shows the microstructure of the same material subjected to heating of 900°C x 10,000 hours (test material No. 2).
  • the second phase is coarsened compared to that shown in FIG. 2 (test material No. 1) due to heating at 900°C x 10,000 hours.
  • the second phase is not only coarser than the second phase shown in FIG. 2 but also has a more rounded shape.
  • test material No 2 which corresponds to the microstructure shown in FIG. 3, are greatly reduced compared with the unheated test material No. 1, which corresponds to the microstructure shown in FIG. 2.
  • the test material No 2 was subjected to the two-stage solution treatment and ageing of the present invention (test material No 7) and which produces a microstructure as shown in FIG. 1 together with full recovery of the mechanical properties as shown in Tables 4 and 5.
  • Test material No. 2 was subjected to the first-stage solution treatment, in which the material is held at a temperature of 1120°C, 1150°C and 1200°C for 2 hours and then is air-cooled, and thereafter was subjected to the aging treatment, in which the material is held at a temperature 850°C for 24 hours and then is air-cooled (test materials Nos. 3, 4 and 5).
  • the microphotographs of x5000 magnification of these materials are shown in FIGS. 4 to 6, and the hardness and tensile test results thereof are shown in Table 4.
  • the second phase, in which the particle is coarsened, of FIG. 3 is scarcely homogenized, and the second phase with a diameter of 0.05 ⁇ m or smaller is slightly re-deposited.
  • the second phase with a diameter of 0.08 ⁇ m or smaller is re-deposited in slightly large numbers.
  • all of the second phases, in which the particle is coarsened are homogenized, and only the second phase with a diameter of 0.1 ⁇ m or smaller is re-deposited in large numbers.
  • the ductility (elongation) of the test materials Nos. 3, 4 and 5 having these microstructures is 3.5%, 2.9% and 2.7%, respectively, which ductility is not recovered to 7.1%, the value of the unheated material.
  • test material No. 2 the material subjected to heating of 900°C x 10,000 hours (test material No. 2) was subjected to two-stage solution treatment of 1200°C x 2 hr/furnace cooling + 1120°C x 2 hr/air cooling (after being held at 1200°C for 2 hours, the material is furnace-cooled to room temperature, and then heated to 1120°C again and held for 2 hours, thereafter being air-cooled to room temperature), which is a treatment method of the present invention, and then subjected to the aging treatment of 850°C x 24 hr/air cooling.
  • the microphotograph of x5000 magnification of this treated material (test material No. 7) is shown in FIG.
  • Test material No. 6 in Table 3 is, like No.7 which is the material of the present invention, subjected to two-stage solution treatment and aging treatment, so that the degree of recovery is higher than that of the materials subjected to one-stage solution treatment as shown in Tables 4 and 5.
  • the first-stage solution treatment temperature is as low as 1150°C, the recovery of ductility is still insufficient.
  • the hardness was HV384, and the tensile strength and elongation at room temperature were 87.2 kg/mm 2 and 7.8%, respectively.
  • the hardness decreased to HV325, and the tensile strength and elongation at room temperature decreased to 81.5 kg/mm 2 and 1.7%, respectively.
  • the 0.2% proof stress and the reduction of area at room temperature and the 0.2% proof stress, tensile strength, elongation, and reduction of area at 650°C also decreased as compared with those of the unheated material.
  • test material No. 9 The heated material (test material No. 9) subjected to heating of 900°C x 10,000 hours, whose strength and ductility have decreased as described above, was, as in the case of alloy A, subjected to two-stage solution treatment and aging treatment to prepare test material No. 11.
  • test material No. 11 hardness test, tensile test, and creep rupture test were conducted.
  • Test material No. 10 in Table 3 is, like No.11 which is the material of the present invention, subjected to two-stage solution treatment. As shown in Tables 6 and 7, since the first-stage solution treatment temperature is as low as 1150°C, the recovery of ductility is still insufficient. Results of creep rupture test of alloy A Test material Test conditions Creep rupture properties No.

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Claims (2)

  1. Verfahren zur Wiederherstellung von Eigenschaften einer hitzebeständigen Legierung auf Ni-Basis, bei dem eine hitzebeständige Legierung auf Ni-Basis, die in Gewichtsprozent 13,1-15% Cr, 8,5-10,5% Co, 1-3,5% Mo, 3,5-4,5% W, 3-5,5% Ta, 3,5-4,5% Al, 2,2-3,2% Ti, 0,06-0,12% C, 0,025% oder weniger B, 0,01-0,05% Zr, 1-100 ppm Mg und/oder Ca, und 0-1,5% Hf enthält, wobei der Rest Ni und unvermeidbare Verunreinigungen aufweist, und deren Eigenschaften durch Wärmeeinwirkung beeinträchtigt wurden, in einer ersten Stufe einer Lösungsbehandlung unterzogen wird, bei der die Legierung während 1 bis 5 Stunden bei einer Temperatur von 1175 bis 1225°C gehalten und dann ofengekühlt wird, anschließend in einer zweiten Stufe einer Lösungsbehandlung unterzogen wird, bei der die Legierung während 1 bis 5 Stunden bei einer Temperatur von 1115 bis 1165°C gehalten und dann luftgekühlt wird, und ferner einer Alterungsbehandlung unterzogen wird, bei der die Legierung während 22 bis 26 Stunden bei einer Temperatur von 810 bis 860°C gehalten wird.
  2. Verfahren zur Wiederherstellung von Eigenschaften einer hitzebeständigen Legierung auf Ni-Basis, bei dem eine hitzebeständige Legierung auf Ni-Basis, die in Gewichtsprozent 15,7-16,3% Cr, 8-9% Co, 1,5-2% Mo, 2,4-2,8% W, 1,5-2% Ta, 3,2-3,7% Al, 3,2-3,7% Ti, 0,09-0,13% C, 0,007-0,012% B, 0,03-0,08% Zr, 0,6-1,1% Nb, 0,05% oder weniger Fe, 0,02% oder weniger Mn, 0,3% oder weniger Si und 0,015% oder weniger S (wobei Al + Ti: 6,5-7,2% beträgt) enthält, wobei der Rest Ni und unvermeidbare Verunreinigungen aufweist, und deren Eigenschaften durch Wärmeeinwirkung beeinträchtigt wurden, in einer ersten -Stufe einer Lösungsbehandlung unterzogen wird, bei der die Legierung während 1 bis 5 Stunden bei einer Temperatur von 1175 bis 1225°C gehalten und dann ofengekühlt wird, anschließend in einer zweiten Stufe einer Lösungsbehandlung unterzogen wird, bei der die Legierung während 1 bis 5 Stunden bei einer Temperatur von 1115 bis 1165°C gehalten und dann luftgekühlt wird, und ferner einer Alterungsbehandlung unterzogen wird, bei der die Legierung während 22 bis 26 Stunden bei einer Temperatur von 810 bis 860°C gehalten wird.
EP99301222A 1998-02-23 1999-02-19 Verfahren zur Wiederherstellung von Eigenschaften einer hitzebeständigen Legierung auf Nickelbasis Expired - Lifetime EP0937784B1 (de)

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JP5574098 1998-02-23
JP05574098A JP3722975B2 (ja) 1998-02-23 1998-02-23 Ｎｉ基耐熱合金の性能回復処理方法

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CA (1) CA2262278C (de)
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CA2287116C (en) * 1999-10-25 2003-02-18 Mitsubishi Heavy Industries, Ltd. Process for the heat treatment of a ni-base heat-resisting alloy
EP1442151B8 (de) 2001-11-09 2011-10-12 Alstom Technology Ltd Wärmebehandlungsverfahren für werkstoffkörper aus einer nickel-basis-superlegierung
EP1398393A1 (de) 2002-09-16 2004-03-17 ALSTOM (Switzerland) Ltd Verfahren zur Wiederherstellung von Eigenschaften
JP4036091B2 (ja) * 2002-12-17 2008-01-23 株式会社日立製作所 ニッケル基耐熱合金及びガスタービン翼
JP4167242B2 (ja) * 2005-04-11 2008-10-15 三菱重工業株式会社 Ｎｉ基耐熱合金の性能回復処理方法
WO2011047714A1 (de) * 2009-10-20 2011-04-28 Siemens Aktiengesellschaft Legierung zur gerichteten erstarrung und bauteil aus stängelförmigen kristallen
US9528175B2 (en) * 2013-02-22 2016-12-27 Siemens Aktiengesellschaft Pre-weld heat treatment for a nickel based superalloy
JP6245728B2 (ja) * 2013-03-27 2017-12-13 三菱重工業株式会社 疲労寿命回復熱処理方法
US10625357B2 (en) * 2017-05-26 2020-04-21 Siemens Energy, Inc. Braze repair of turbomachine engine component
CN108913952B (zh) * 2018-07-27 2020-04-03 南京工程学院 一种高温合金及其制备方法
US11795832B2 (en) 2019-11-13 2023-10-24 Siemens Energy, Inc. System and method for repairing high-temperature gas turbine components
CN111621728B (zh) * 2020-07-01 2021-07-20 中南大学 一种均匀细化固溶态gh4169合金锻件混晶组织的方法
US11712738B2 (en) * 2021-01-28 2023-08-01 Siemens Energy, Inc. Crack healing additive manufacturing of a superalloy component
CN116083753A (zh) * 2022-12-22 2023-05-09 哈尔滨汽轮机厂有限责任公司 一种可用于750℃超超临界汽轮机高温叶片用Ni基合金材料
CN119588960A (zh) * 2024-12-10 2025-03-11 有研增材技术有限公司 一种用于增材制造gh4099合金的热处理方法
CN119956273B (zh) * 2025-01-17 2026-04-21 北京科技大学 一种修复镍基单晶合金蠕变损伤的亚固溶恢复热处理方法

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US6171417B1 (en) 2001-01-09
DE69900654D1 (de) 2002-02-21
DE69900654T2 (de) 2002-10-02
EP0937784A1 (de) 1999-08-25
JPH11236655A (ja) 1999-08-31
CA2262278C (en) 2002-09-10
JP3722975B2 (ja) 2005-11-30
CA2262278A1 (en) 1999-08-23

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